WO2007142175A1 - 接合方法 - Google Patents

接合方法 Download PDF

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Publication number
WO2007142175A1
WO2007142175A1 PCT/JP2007/061266 JP2007061266W WO2007142175A1 WO 2007142175 A1 WO2007142175 A1 WO 2007142175A1 JP 2007061266 W JP2007061266 W JP 2007061266W WO 2007142175 A1 WO2007142175 A1 WO 2007142175A1
Authority
WO
WIPO (PCT)
Prior art keywords
joining
powder
metal
bonding
metal powder
Prior art date
Application number
PCT/JP2007/061266
Other languages
English (en)
French (fr)
Inventor
Toshinori Ogashiwa
Masayuki Miyairi
Original Assignee
Tanaka Kikinzoku Kogyo K.K.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Tanaka Kikinzoku Kogyo K.K. filed Critical Tanaka Kikinzoku Kogyo K.K.
Priority to CN2007800008088A priority Critical patent/CN101341585B/zh
Priority to EP07744651.6A priority patent/EP1916709A4/en
Priority to US12/063,264 priority patent/US7789287B2/en
Publication of WO2007142175A1 publication Critical patent/WO2007142175A1/ja

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Definitions

  • the present invention relates to a method for joining a pair of joining members at a relatively low temperature. Specifically, the present invention relates to a method for performing die bonding and flip chip bonding of a chip to a substrate at a low temperature.
  • brazing method power using brazing material Widely used as a joining method for various members.
  • flux-less brazing material is used to prevent component contamination in order to die-bond to semiconductor chip substrates used in high-frequency and optical modules, and AuSn brazing material is used as such brazing material.
  • Patent Document 1 For example, Patent Document 1,
  • Patent Document 1 JP 2004-006521 A
  • the brazing material is fused to one joining member (for example, a semiconductor chip) and then placed on the other joining member (for example, a substrate).
  • the brazing filler metal is melted and solidified by heating to a temperature above the melting point of the brazing material.
  • the bonding temperature is often set to a temperature of 300 ° C or higher in consideration of the melting point of the brazing material used (the melting point of the AuSn brazing material is about 280 ° C).
  • the bonding temperature is set high, the thermal stress generated when cooling to room temperature after bonding increases, and there is a concern about the influence on the bonding member.
  • the electrical characteristics of the semiconductor chip may vary due to thermal stress. Therefore, depending on the joining member, a method is desired in which the joining temperature is as low as possible in order to reduce thermal stress.
  • the present invention has been made based on the background as described above, and an object thereof is to provide a bonding method having sufficient bonding strength at a relatively low temperature. Specifically, it provides a method that enables bonding even at temperatures below 300 ° C.
  • the inventors of the present invention have studied a joining method that replaces the conventional brazing that can solve the above-described problems. As a result of the investigation, a bonding method using a metal paste having a predetermined configuration was found.
  • the present invention is a method for joining a pair of joining members, including the following steps.
  • the joining method according to the present invention is a joining method using a metal paste instead of the brazing material.
  • the metal paste applied to the joining member is pressurized while being heated, and thereby the metal powder in the paste is joined while being plastically deformed to form a dense joint and joining is performed.
  • the paste is sintered before pressing to obtain a metal powder sintered body.
  • the metal paste used in the present invention is a gold powder, silver powder, platinum powder, or palladium having a purity of 99.9% by weight or more and an average particle diameter of 0.005 / ⁇ ⁇ to 1.0 m.
  • a mixture of one or more metal powders selected from powder and an organic solvent is used.
  • the purity of the metal powder is required to be as high as 99.9% by weight because if the purity is low, the hardness of the powder increases and plastic deformation becomes difficult.
  • the average particle size of the metal powder 1.
  • a metal powder having a particle size exceeding O 2 / zm is difficult to express a preferable proximity state during sintering described later.
  • the lower limit of 0.005 m is to consider that when the particle size is less than this particle size, it aggregates and becomes difficult to handle immediately when made into a paste.
  • the powder power of any of gold, silver, platinum or palladium is When used for bonding semiconductor chips, such as soldering, the metal paste is also required to have electrical conductivity. These metals have excellent electrical conductivity.
  • ester alcohol As the organic solvent constituting the metal paste, ester alcohol, tervineol, pine oil, butyl carbitol acetate, butyl carbitol and carbitol are preferable.
  • ester alcohol-based organic solvent 2,2,4-trimethyl-1-hydroxypentaisobutyrate (C 3 H 2 O 3) can be mentioned.
  • the metal paste may contain one or more selected from acrylic resin, cellulose resin, and alkyd resin. If these fats and the like are further added, the metal powder in the metal paste is prevented from agglomerating and becomes more homogeneous.
  • acrylic resin include methyl methacrylate polymer
  • examples of the cellulose resin include ethyl cellulose
  • examples of the alkyd resin include phthalic anhydride resin. Of these, ethylcellulose is particularly preferred.
  • a method of applying the metal paste to the bonding member various methods can be used depending on the size of the bonding portion, such as a spin coating method, a screen printing method, an ink jet method, and a method of spreading the paste with a spatula after dropping. Can be used.
  • the reason for drying the applied metal paste is to remove the organic solvent in the paste. This drying is preferably performed at -20 ° C or higher and 5 ° C or lower.
  • the atmosphere in the drying process may be a reduced pressure atmosphere. This prevents moisture in the atmosphere from condensing on the metal powder surface during the drying process.
  • the force is preferably 1 OOPa or less, more preferably lOPa or less.
  • the degree of vacuum in this atmosphere is set according to the volatility of the organic solvent in the metal paste.
  • the metal particles in the paste and the bonding surface (paste application surface) of the bonding member and the metal particles are in close contact with each other, and the metal paste becomes a metal powder sintered body.
  • This metal powder sintered body is heated and pressed at the time of joining, which will be described later, so that plastic deformation occurs at the contact portion, and bonds between metal atoms occur at the deformation interface, and the sintered body is densely joined. Part. In this regard, even if the paste is pressed without sintering, the particle gaps are expanded. , Bonding between particles does not occur and bonding is not possible.
  • the sintering temperature is 80 to 300 ° C. This is because the above point contact does not occur below 80 ° C. On the other hand, if sintering at a temperature exceeding 300 ° C, sintering proceeds excessively, necking between the metal powders proceeds and bonds firmly, and even if pressed after that, it does not become a dense joint. In particular, the strain tends to remain during pressurization. In the first place, the present invention aims at joining at 300 ° C. or lower from the viewpoint of protecting the joining member.
  • the heating time during sintering is preferably 30 to 120 minutes.
  • this sintering is preferably performed in a state where no pressure is applied.
  • the joining member to which the metal paste is applied and the other joining member are stacked and pressed.
  • the pressurizing pressure is preferably larger than the yield strength of the metal powder sintered body for densification of the joint. Further, this pressurization may be performed in one direction from any of the joining members, or a bidirectional force may be performed.
  • the joining step it is necessary to pressurize the metal powder sintered body while heating it. Without heating, the joint is not sufficiently densified and the strength of the joint is insufficient.
  • the heating temperature at this time is preferably 80 to 300 ° C. This is because bonding is not possible at temperatures below 80 ° C, and thermal strain at the time of cooling increases at temperatures above 300 ° C.
  • the bonding step it is preferable to apply ultrasonic waves in addition to heating.
  • ultrasonic waves By heating or a combination of heating and ultrasonic waves, plastic deformation and bonding of the metal powder can be promoted and a stronger joint can be formed.
  • the conditions are preferably an amplitude of 0.5 to 5 / ⁇ ⁇ and an application time of 0.5 to 3 seconds. This is because application of excessive ultrasonic waves damages the joining member.
  • the heating and the application of ultrasonic waves in the joining step may be performed on the sintered power of at least the metal powder, but may be performed on the entire joining member.
  • a heating method it is easy to use heat transfer with a tool force when pressurizing the joining member.
  • ultrasonic waves it is easy to apply ultrasonic waves to oscillate the tool force for pressurizing the joining member.
  • FIG. 1 is a diagram schematically illustrating a bonding process in the present embodiment.
  • FIG. 2 Structure observation results of sintered metal powder sintered body and joint after joining.
  • FIG. 3 is a diagram showing the structure of a sintered metal powder when sintering is performed at 400 ° C.
  • FIG. 4 is a diagram showing a test method for bonding strength.
  • FIG. 1 schematically shows a bonding process of a semiconductor chip (GaAs chip) to a substrate performed in this embodiment.
  • GaAs chip semiconductor chip
  • Example 1 First, a metal paste 20 was applied to a semiconductor chip 10.
  • the surface of the semiconductor chip 10 is pre-fixed with Ti (0.5 / ⁇ ⁇ ), Ni d / z m ⁇ (1 / ⁇ ⁇ ), Pd d / z m).
  • the metal paste used is gold powder (average particle size: 0.3 m) with a purity of 99.99% by weight produced by a wet reduction method, and ester alcohol (2, 2, 4-trimethyl 3-hydroxy) as an organic solvent. It is prepared by mixing pentaisobutyrate (CHO))
  • the metal paste had an area of 0.0033 mm 2 and was applied at 100 locations on the chip.
  • the metal paste 20 was applied, it was vacuum dried at -10 ° C with a dryer. Then, the chip was heated in an electric furnace at 230 ° C. for 30 minutes to sinter the metal paste to obtain a powder metal sintered body 21.
  • a Ni plate 30 pre-plated with Au (: m), Pd (: m) was placed on the semiconductor chip 10 and joined by heating and pressing.
  • the pressure condition at this time was 0.2 N per sintered body.
  • the heating was set to 230 ° C due to the heat transfer of the tool.
  • the heating and pressurizing time in this joining process was 10 minutes.
  • Example 2 Here, joining was performed by applying ultrasonic waves simultaneously with pressurization and heating of the sintered bodies.
  • a metal paste was applied to a semiconductor chip * dried, sintered, and then a Ni plate was placed thereon. Then, heating and pressurization were performed in the same manner as in Example 1 ( Pressurization pressure was 0.33 N per sintered body;).
  • the ultrasonic wave was applied from a tool, the amplitude was 3.2 / ⁇ ⁇ , the output was 3.5 W, and the application time was 1 second.
  • the bonding strength of each example exceeds lOOMPa. Considering the joining of electronic components, it can be said that the joint strength is sufficient. It can also be seen that the bonding strength is improved by using ultrasonic wave application at the time of bonding.
  • various joining members can be joined at a relatively low temperature, and the joining members can be protected from thermal stress in the cooling process after joining.
  • the present invention is useful when bonding a semiconductor chip or the like, which may be affected by thermal stress, to a substrate, and can be applied to die bonding, flip chip bonding, and the like. When applied to flip chip bonding, the present invention can be applied to form bumps on a semiconductor chip.

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Description

接合方法
技術分野
[0001] 本発明は、一対の接合部材を比較的低温で接合するための方法に関する。具体 的には、チップの基板へのダイボンド、フリップチップ接合を低温で行なうための方法 に関する。
背景技術
[0002] ろう材を用いたろう付け法力 各種部材の接合方法として広く用いられている。特に 、高周波 ·光モジュールなどで用いられる半導体チップの基板へダイボンドするため には、部品の汚染を防止するためフラックスレスのろう材が使用されており、そのよう なろう材として AuSn系ろう材が一般に使用されている（例えば、特許文献 1)。
特許文献 1 :特開 2004— 006521号公報
[0003] 通常、ろう材を使用するろう付け法においては、ろう材を一方の接合部材 (例えば、 半導体チップ）に融着した後、これを他方の接合部材 (例えば、基板）に載置して、ろ ぅ材の融点以上の温度に加熱してろう材を溶融'凝固させている。この接合時の温度 は、使用するろう材の融点 (AuSn系ろう材の融点は約 280°Cである）を考慮して 300 °C以上の温度に設定されることが多い。
発明の開示
発明が解決しょうとする課題
[0004] し力しながら、接合温度を高温とすると、接合後、常温へ冷却する際に生じる熱応 力が大きくなり、その接合部材への影響が懸念される。例えば、半導体チップのダイ ボンドにおいては、熱応力により半導体チップの電気的特性の変動が生じるおそれ がある。従って、接合部材によっては、熱応力の低減のため接合温度ができるだけ低 い方法が望まれる。本発明は、以上のような背景のもとになされたものであり、比較的 低温で十分な接合強度を有する接合方法を提供することを目的とする。具体的には 300°C以下の温度でも接合可能な方法を提供する。
課題を解決するための手段 [0005] 本発明者等は、上記課題を解決すベぐ従来のろう付けに替わる接合方法の検討 を行った。そして、検討から、所定の構成を有する金属ペーストを使用する接合方法 を見出した。
[0006] 即ち、本発明は、一対の接合部材を接合する方法において、下記工程を含むこと を特徴とする方法である。
(a)—方の接合部材に、純度が 99. 9重量％以上であり、平均粒径が 0. 005 μ m~ 1. O /z mである金粉、銀粉、白金粉、又はパラジウム粉から選択される一種以上の金 属粉末と、有機溶剤とからなる金属ペーストを塗布する工程。
(b)前記金属ペーストを乾燥し、 80〜300°Cの温度で焼結させて金属粉末焼結体と する工程。
(c)前記金属粉末焼結体を介して前記一方の接合部材と他方の接合部材とを配置 し、少なくとも金属粉末焼結体を加熱しながら一方向又は双方向から加圧して接合 する工程。
[0007] 本発明に係る接合方法は、ろう材に替えて金属ペーストを使用する接合方法である 。この方法では、接合部材に塗布された金属ペーストを加熱しながら加圧し、これに よりペースト中の金属粉末を塑性変形させつつ結合させ密な接合部を形成して接合 を行なう。そして、接合工程での金属粉末の結合を容易に進行させるため、加圧の 前にペーストを焼結して金属粉末焼結体とするものである。以下、本発明に係る方法 について、より詳細に説明する。
[0008] 本発明において使用する金属ペーストとしては、純度が 99. 9重量％以上であり、 平均粒径が 0. 005 /ζ πι〜1. 0 mである金粉、銀粉、白金粉、又はパラジウム粉か ら選択される一種以上の金属粉に、有機溶剤を混合したものが用いられる。金属粉 の純度について 99. 9重量％以上の高純度を要求するのは、純度が低いと粉末の 硬度が上昇し、塑性変形し難くなるからである。また、金属粉の平均粒径については 、 1. O /z mを超える粒径の金属粉では、後述する焼結の際、好ましい近接状態を発 現させ難くなるからである。一方、 0. 005 mを下限とするのはこの粒径未満の粒径 では、ペーストとしたときに凝集しやすぐ取扱いが困難となることを考慮するものであ る。尚、金、銀、白金、又はパラジウムのいずれかの粉末力もなるのは、ダイボンディ ング等の半導体チップの接合に使用する場合には、金属ペーストにも導電性が要求 される力 これらの金属は導電性が良好だ力もである。
[0009] 金属ペーストを構成する有機溶剤としては、エステルアルコール、タービネオール、 パインオイル、ブチルカルビトールアセテート、ブチルカルビトール、カルビトールが 好ましい。例えば、好ましいエステルアルコール系の有機溶剤として、 2, 2, 4ートリメ チル一 3—ヒドロキシペンタイソブチレート（C H O )、を挙げることができる。これら
12 24 3
の溶剤は、比較的低温で乾燥させることができるからである。
[0010] 尚、金属ペーストは、アクリル系榭脂、セルロース系榭脂、アルキッド榭脂から選択 される一種以上を含有して 、ても良 、。これらの榭脂等を更にカ卩えると金属ペースト 中の金属粉の凝集が防止されてより均質となる。尚、アクリル系榭脂としては、メタタリ ル酸メチル重合体を、セルロース系榭脂としては、ェチルセルロースを、アルキッド榭 脂としては、無水フタル酸榭脂を、それぞれ挙げることができる。そして、これらの中 でも特にェチルセルロースが好まし 、。
[0011] 金属ペーストを接合部材に塗布する方法としては、スピンコート法、スクリーン印刷 法、インクジェット法、ペーストを滴下後にヘラ等で広げる方法等、接合部の大きさに 対応させて種々の方法を用いることができる。
[0012] 塗布した金属ペーストを乾燥させるのは、ペースト中の有機溶剤を除去するためで ある。この乾燥は、— 20°C以上 5°C以下で行なうのが好ましい。乾燥工程における雰 囲気を減圧雰囲気としても良い。これにより乾燥過程において大気中の水分が金属 粉末表面に結露するのを防止することができる。減圧雰囲気とする場合、好ましくは 1 OOPa以下、より好ましくは lOPa以下とする力 この雰囲気の真空度は、金属ペース ト中の有機溶剤の揮発性に応じて設定する。
[0013] 本発明では、金属ペーストを塗布 '乾燥した後に焼結することを要する。これにより 、ペースト中の金属粒子同士、及び接合部材の接合面 (ペースト塗布面）と金属粒子 との間に、互いに点接触した近接状態が形成され、金属ペーストは金属粉末焼結体 となる。この金属粉末焼結体は、後述の接合時で加熱'加圧されることで、接触部に 塑性変形が生じると共に、その変形界面で金属原子間の結合が生じ、焼結体は緻密 な接合部となる。この点、焼結することなしにペーストを加圧しても粒子間隙が広がり 、粒子同士の結合が生ぜず接合ができない。
[0014] この焼結の温度は、 80〜300°Cとする。 80°C未満では上記のような点接触が生じ ないからである。一方、 300°Cを超える温度で焼結すると、焼結が過度に進行し、金 属粉末間のネッキングが進行して強固に結合してしまい、その後に加圧しても緻密な 接合部にならないことにカ卩え、加圧の際に歪が残留し易くなるからである。また、そも そも本発明は、接合部材を保護する観点から 300°C以下での接合を目指すものだか らである。尚、焼結の際の加熱時間は、 30〜 120分とするのが好ましい。短時間では 焼結炉の温度が安定せず十分な焼結ができず、また、あまりに長時間とすると生産 性が損なわれるからである。また、この焼結は、圧力の負荷のない状態で行なうのが 好ましい。
[0015] 上記焼結を行った後の加圧による接合は、金属ペーストを塗布した接合部材と、他 方の接合部材とを重ねて加圧する。加圧の圧力は、接合部の緻密化のため、金属粉 末焼結体の降伏強度より大きくするのが好ましい。また、この加圧は、いずれかの接 合部材から一方向で行っても良いし、双方向力も行っても良い。
[0016] そして、この接合工程の際には、金属粉末焼結体を加熱しながら加圧することが必 要である。加熱しない場合、接合部の緻密化が不十分となり、接合強度が不足する 力もである。このときの加熱温度は、 80〜300°Cとするのが好ましい。 80°C未満では 接合ができないからであり、 300°Cを超えると冷却時の熱歪の影響が大きくなるから である。
[0017] また、接合工程においては、加熱に加えて超音波を印加するのが好ましい。加熱 又は加熱と超音波との組合わせにより、金属粉末の塑性変形及び結合を促進し、よ り強固な接合部を形成することができる。超音波を印加する場合、その条件は、振幅 0. 5〜5 /ζ πιとし、印加時間を 0. 5〜3秒とするのが好ましい。過大な超音波印加は 接合部材を損傷させるからである。
[0018] 接合工程における上記加熱及び超音波印加は、その目的力 少なくとも金属粉末 焼結体に対して行なえばよいが、接合部材全体に行っても良い。加熱の方法として は、接合部材を加圧する際の工具力もの伝熱を利用するのが簡易である。同様に、 超音波の印加は、接合部材を加圧する工具力も超音波発振させるのが簡易である。 図面の簡単な説明
[0019] [図 1]本実施形態における接合工程を概略説明する図。
[図 2]焼結後の金属粉末焼結体及び接合後の接合部の組織観察結果。
[図 3]焼結を 400°Cで行なったときの金属粉末焼結体の組織を示す図。
[図 4]接合強度の試験方法を示す図。
発明を実施するための最良の形態
[0020] 以下、本発明の好適な実施形態を説明する。図 1は、本実施形態で行った、半導 体チップ (GaAsチップ)の基板への接合工程を概略示すものである。以下、図を参 照しつつ各実施例における接合工程について説明する。
[0021] 実施例 1 :まず、半導体チップ 10に金属ペースト 20を塗布した。半導体チップ 10は、 その表面に、 Ti(0. 5 /ζ πι)、 Ni d /z m Αιι (1 /ζ πι)、 Pd d /z m)を予めめつきして いる。使用する金属ペーストは、湿式還元法により製造された純度 99. 99重量％の 金粉 (平均粒径: 0. 3 m)と、有機溶剤としてエステルアルコール（2, 2, 4—トリメチ ルー 3—ヒドロキシペンタイソブチレート（C H O ) )を混合して調整されたものであ
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る。金属ペーストは面積 0. 0034mm2で、チップ上に 100箇所塗布した。
[0022] 金属ペースト 20を塗布した後、これを乾燥器にて— 10°Cで真空乾燥した。そして、 チップを電気炉にて、 230°Cで 30分加熱して金属ペーストを焼結し、粉末金属焼結 体 21とした。
[0023] 焼結処理後、 Ni板 30 (Au (： m)、 Pd (： m)を予めめつきしたもの）を、半導体 チップ 10の上に載置し、加熱及び加圧して接合した。このときの加圧条件は、一つ の焼結体当り 0. 2Nとした。また、加熱は工具力もの伝熱により 230°Cとなるようにし た。この接合工程での加熱及び加圧時間は、 10分間とした。
[0024] 実施例 2 :ここでは、焼結体の加圧'加熱と同時に超音波印加を行い接合した。実施 例 1と同様にして、半導体チップに金属ペーストを塗布 *乾燥し、焼結を行った後、こ れに Ni板を載置し、実施例 1と同様に過熱'加圧を行った (加圧の圧力は一つの焼 結体当り 0. 33Nとした。；)。超音波は、工具より印加し、振幅 3. 2 /ζ πι、出力 3. 5W、 印加時間は 1秒とした。
[0025] 以上の各実施例において、焼結を行った後の金属粉末焼結体、及び、接合後の接 合部の組織についての観察結果を図 2に示す。図からわ力るように、焼結により、金 属粉末は点接触に近い状態で近接している。そして、その後の加圧及び加熱により 緻密な組織を示す。特に、超音波を印加することにより、内部は微細な結晶組織を示 すことがわかる。尚、本実施形態の予備的試験として、焼結を 400°Cで行なったとき の金属粉末焼結体の組織を図 3に示すが、焼結温度を 400°Cとすることで金属粒子 の結合が進行しているのがわかる。そして、この状態で加圧を行なったところ、接合が 不可能であった。つまり、接合前の焼結を適切に行うことが必要である。
[0026] 次に、各実施例で行った接合に関して、接合強度の検討を行った。この検討は、図 4で示すように、横方向から一定速度でブレードをチップに当接、進行させ、破断 (チ ップの剥離)が生じたときの応力を測定し、この値と破断後の接合部面積とから単位 面積あたりの強度を算出した。この結果を表 1に示す。
[0027] [表 1]
Figure imgf000008_0001
[0028] 表 1から、各実施例による接合強度は、いずれも lOOMPaを超えている。電子部品 の接合等を考慮すれば十分な接合強度といえる。また、接合強度は、接合時に超音 波印加を併用することにより、向上することがわかる。
産業上の利用可能性
[0029] 以上説明したように、本発明によれば、各種の接合部材を比較的低温で接合する ことができ、接合後の冷却過程における熱応力から接合部材を保護することができる 。本発明は、熱応力の影響が懸念される半導体チップ等を基板へ接合する際に有 用であり、そのダイボンディング、フリップチップ接合等へ適用することができる。尚、 フリップチップ接合に適用するに当たっては、半導体チップのバンプ形成のために本 発明を適用することができる。

Claims

請求の範囲
[1] 一対の接合部材を接合する方法にぉ ヽて、下記工程を含むことを特徴とする方法。
(a)—方の接合部材に、純度が 99. 9重量％以上であり、平均粒径が 0. 005 μ m~ 1. である金粉、銀粉、白金粉、又はパラジウム粉から選択される一種以上の金 属粉末と、有機溶剤とからなる金属ペーストを塗布する工程。
(b)前記金属ペーストを乾燥し、 80〜300°Cの温度で焼結させて金属粉末焼結体と する工程。
(c)前記金属粉末焼結体を介して前記一方の接合部材と他方の接合部材とを配置 し、少なくとも金属粉末焼結体を加熱しながら一方向又は双方向から加圧して接合 する工程。
[2] (c)工程での加熱温度を 80〜300°Cとする請求項 1記載の接合方法。
[3] (c)工程で、更に、少なくとも金属粉末焼結体に超音波を印加して加圧する請求項 1 又は請求項 2記載の接合方法。
PCT/JP2007/061266 2006-06-05 2007-06-04 接合方法 WO2007142175A1 (ja)

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EP1916709A1 (en) 2008-04-30
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